CN108225972B - Apparatus and method for determining the size of a leak in a sample - Google Patents

Apparatus and method for determining the size of a leak in a sample Download PDF

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CN108225972B
CN108225972B CN201810053504.8A CN201810053504A CN108225972B CN 108225972 B CN108225972 B CN 108225972B CN 201810053504 A CN201810053504 A CN 201810053504A CN 108225972 B CN108225972 B CN 108225972B
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CN108225972A (en
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希尔瑞·戈塞
菲利普·拉萨尔瑞
埃里克·沙勒
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ANEOLIA
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/26—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors
    • G01M3/32—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F5/00—Measuring a proportion of the volume flow
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F9/00—Measuring volume flow relative to another variable, e.g. of liquid fuel for an engine
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/007—Leak detector calibration, standard leaks
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/10—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing diffusion of components through a porous wall and measuring a pressure or volume difference
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/14—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature
    • G01N27/18—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature caused by changes in the thermal conductivity of a surrounding material to be tested

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Abstract

The invention relates to a device (1) for testing a sample (13) by means of a gas flow, comprising: an opening (2); means (3) for generating an airflow (25) in the apparatus along at least one flow path through the opening; at least one pressure sensor (5, 6), each pressure sensor being arranged to measure the pressure of the gas flow along at least one flow path; and a mass flow meter (4) arranged to measure a parameter representative of the mass flow rate of the gas flow along the flow path. According to the invention, the device is arranged to quantify the presence of a gas of interest in the gas to be analyzed and/or to determine the size of the leak orifice (22) by means of a measured value of a parameter representative of the mass flow rate. The invention also relates to a method implemented by such a device. The method may be used to test the integrity of food packaging, as well as to test for leaks or problems associated with sealed containers.

Description

Apparatus and method for determining the size of a leak in a sample
The present application is a divisional application of chinese application No. 201380073513.9 entitled "apparatus and method for differentiating gases in a sample", filed on 19/12/2013.
Technical Field
The present invention relates to an apparatus for testing a sample. The invention also relates to a method implemented by the device.
The apparatus allows a user to test a sample, for example, to cause dynamic stress to be generated in the sample by dynamic countercurrent flow, and/or to measure the integrity of the sample enclosure, and/or to measure the gas permeability of the sample, and/or to distinguish between gases in the sample, etc.
Background
Systems for testing samples are known, for example, systems for measuring the proportion of a given gas within a sample, or systems for measuring leaks or problems associated with the sealing of a sample.
A common drawback of the prior art solutions is that these solutions are too expensive and time consuming (for CO)2Typical response time for infrared measurements of the scale is 12 seconds) or not accurate enough (the smallest measurable dimension of the leak is 5 μm and has a relative excess pressure of 500mbar or helium flush in the enclosure is measured).
The object of the present invention is to propose a device and a method for testing a sample, which have at least one of the following technical advantages:
low production costs with respect to the prior art,
high measurement speed with respect to the prior art,
high measurement resolution with respect to the prior art.
Disclosure of Invention
This object is achieved by a device for testing a sample by means of a gas flow, comprising:
-an opening for the passage of the fluid,
-means for generating an airflow in the device along at least one flow path through the opening,
-at least one pressure sensor, each pressure sensor being arranged to measure the pressure of the gas flow along at least one flow path, an
-a mass flow meter arranged to measure a parameter representative of the mass flow rate of the gas flow along each flow path.
A first aspect of the apparatus according to the invention:
the at least one flow path may comprise an inhalation path starting from the opening,
the means for generating a gas flow may be arranged to suck in the gas to be analyzed, so that the gas to be analyzed flows along the suction path,
in the device, the above-mentioned suction path can be locally narrowed at the measuring aperture,
the at least one pressure sensor may comprise a suction pressure sensor arranged to measure the pressure of the gas to be analyzed along the suction path,
the mass flow meter may be arranged to measure a parameter representative of the mass flow rate of the gas to be analysed along the suction path, an
The apparatus may further comprise computing means arranged to quantify the presence of a gas of interest in the gas to be analysed on the basis of a measured value of a parameter representative of the mass flow rate of the gas to be analysed along the inhalation path.
The mass flow meter is preferably a mass flow meter utilizing thermal conductivity.
The calculation means may be arranged to quantify the presence of the gas of interest in the form of a calculation of the proportion of the gas of interest, wherein the calculation is dependent on the diameter of the measurement aperture.
The suction pressure sensor may be disposed along a suction path between the opening and the measurement hole.
The mass flow meter may be disposed along the suction path such that the measuring orifice is disposed along the suction path between the opening and the mass flow meter.
The calculation means may be arranged to quantify the presence of the gas of interest in the form of a calculation of the proportion of the gas of interest, wherein the calculation:
-affine dependence on the square root of a parameter representing the mass flow rate along the suction path, or
-affine dependent on a parameter representative of the mass flow rate along the suction path.
The calculation means may be arranged to quantify the presence of the gas of interest also on the basis of a measurement of the pressure along the suction path measured by the suction pressure sensor, the calculation means may be arranged to quantify the presence of the gas of interest in the form of a calculation of a proportion of the gas of interest, wherein the calculation:
-the inverse of the fourth square root which depends affine on the measurement of the pressure along the suction path measured by the suction pressure sensor: the computing means may be arranged to operate in accordance with a formula
Figure BDA0001553037020000031
Quantifying the presence of the gas of interest in the form of calculating a proportion of the gas of interest, wherein DmIs a parameter representing the mass flow rate, PrIs the pressure measured by the suction pressure sensor, a and B are numerical calibration coefficients; or
-the inverse of the measurement of the pressure along the suction path measured by the suction pressure sensor. The computing means may be arranged to operate in accordance with a formula
Figure BDA0001553037020000032
Quantifying the presence of the gas of interest in the form of calculating a proportion of the gas of interest, wherein DmIs a parameter representing the mass flow rate, PrIs the pressure measured by the suction pressure sensor, and M and N are numerical calibration coefficients.
The calculation means may be arranged to trigger a quantification of the presence of the gas of interest for a value of the pressure along the suction path measured by the suction sensor corresponding to a suction pressure reference value, the calculation means being arranged to quantify the presence of the gas of interest on the basis of a value of a parameter representative of the mass flow rate along the suction path measured simultaneously with the pressure measurement, which pressure measurement measures the pressure value corresponding to the suction pressure reference value. The calculation means may be arranged to quantify the presence of the gas of interest in the form of a proportion of the gas of interest calculated according to the following formula:
Figure BDA0001553037020000033
wherein DmIs a parameter representing the mass flow rate, and A and B are numerical calibration coefficients, or
M*Dm+ N, wherein DmIs a representative substanceThe parameters of the volumetric flow rate, M x and N, are numerical calibration coefficients.
The computing means may also be arranged to quantify the presence of a first molecule of interest having a thermal conductivity in the gas of interest, the apparatus further comprising at least one gas sensor along the inhalation path, the gas sensor being arranged to quantify the presence of at least one other molecule of interest in the gas of interest, the molecule having a thermal conductivity that differs from the thermal conductivity of the first molecule of interest by at most 10% (preferably at most 5%) under the same conditions, the computing means being arranged to quantify the presence of the first molecule of interest based on the quantifying the presence of the gas of interest and the quantifying the presence of the other molecule of interest.
The at least one flow path may comprise a dilution path terminating in an opening, whereupon the means for generating a gas flow is arranged to expel dilution gas along the dilution path.
According to a second aspect of the apparatus according to the invention, which may be combined with the first aspect of the apparatus according to the invention:
the at least one flow path may comprise a discharge path terminating in an opening,
the means for generating a gas flow may be arranged to discharge leakage gas along a discharge path,
the at least one pressure sensor may comprise a discharge pressure sensor arranged to measure a pressure of the leaking gas along the discharge path,
the mass flow meter may be arranged to measure a parameter representative of a mass flow rate of the leaking gas along the discharge path, an
The apparatus may further comprise a computing device arranged to determine the size of a leak of the sample connected to the opening based on a measurement of a parameter representative of the mass flow rate along the exit path.
The mass flow meter is preferably a mass flow meter utilizing thermal conductivity.
The exhaust pressure sensor is preferably disposed along the exhaust path between the mass flow meter and the opening.
The calculation means may be arranged to determine the size of the leak in the form of a calculation which is affine dependent on the square root of a parameter representing the mass flow rate along the discharge path.
The calculation means may be arranged to determine the size of the leak hole also on the basis of a measurement of the pressure along the discharge path measured by the discharge pressure sensor. The calculation means may be arranged to determine the size of the leak in the form of a calculation which is affine dependent on the inverse of the fourth root of the measurement of the pressure along the discharge path. The computing means may be arranged to be based on a formula
Figure BDA0001553037020000041
Determining the size of the leak hole, wherein DmIs a parameter representing the mass flow rate, PrIs the pressure measured by the suction pressure sensor, and a and b are numerical calibration coefficients.
The calculation means may be arranged to trigger the determination of the size of the leak for a value of the pressure along the exhaust path measured by the exhaust pressure sensor corresponding to an exhaust pressure reference value, the calculation means being arranged to determine the size of the leak based on a value of a parameter representative of the mass flow rate along the exhaust path measured simultaneously with a pressure measurement measuring a pressure value corresponding to the exhaust pressure reference value. The computing means may be arranged to be based on a formula
Figure BDA0001553037020000042
Determining the size of the leak hole, wherein DmIs a parameter representing mass flow rate, and a and b are numerical calibration coefficients.
The at least one flow path may comprise a calibration path through the opening and within the apparatus, which may narrow locally at the measurement aperture, the computing means preferably being arranged to:
-determining the size of the measurement aperture on the basis of the measured values of a parameter representative of the mass flow rate along the calibration path, and
-adjusting the calibration factor for calculating the size of the leak if it is determined that the size of the measurement hole does not correspond to the actual size of the measurement hole stored by the calculation means.
The apparatus according to the invention may comprise a valve arranged to complete the exhaust path through a short circuit path through the opening and the flow generating means but not through the flow meter, the valve preferably being arranged to regulate the total flow rate through the exhaust path and the short circuit path.
There is also proposed a method for testing a sample by means of a gas flow, preferably implemented in a first aspect of the device according to the invention, characterized in that it comprises:
-aspirating a gas to be analyzed originating from the sample, the gas to be analyzed flowing along an aspiration path starting from an opening in communication with the sample, the aspiration path being locally narrowed at the measurement orifice,
-measuring the pressure of the gas to be analyzed along the suction path,
-measuring a parameter representative of the mass flow rate of the gas to be analyzed along the suction path, and
-quantifying the presence of the gas of interest in the gas to be analyzed based on a measurement of a parameter representative of the mass flow rate along the inhalation path.
The measurement of the parameter representative of the mass flow rate is preferably a measurement by a mass flow meter using thermal conductivity.
Quantification of the presence of the gas of interest includes calculation of the proportion of the gas of interest, which depends on the diameter of the measurement hole.
The measurement of the pressure may be performed by a suction pressure sensor disposed along a suction path between the sample and the measurement hole.
The measurement of the parameter representative of the mass flow rate may be performed by a mass flow meter disposed along the aspiration path such that the measurement orifice is disposed along the aspiration path between the sample and the mass flow meter.
The quantification of the presence of the gas of interest may comprise a calculation of the proportion of the gas of interest, which calculation is affine dependent on the square root of a parameter representing the mass flow rate along the suction path.
Quantification of the presence of the gas of interest may comprise calculation of the proportion of the gas of interest, which calculation is affine dependent on a parameter representative of the mass flow rate along the inhalation path.
Quantification of the presence of the gas of interest may also be performed based on the pressure measured along the suction path. Quantification of the presence of the gas of interest may include calculation of the gas proportion of interest, which is affine dependent on:
-the inverse of the fourth root of the measurement of the pressure along the suction path. Quantifying the presence of the gas of interest may comprise formulating
Figure BDA0001553037020000061
Of the gas of interest, wherein DmIs a parameter representing the mass flow rate, PrIs the measured pressure, a and B are numerical calibration coefficients; or
-pressure P measured along the suction pathrThe reciprocal of (c). Quantifying the presence of the gas of interest may comprise formulating
Figure BDA0001553037020000062
Of the gas of interest, wherein DmIs a parameter representing the mass flow rate, PrIs the measured pressure, and M and N are numerical calibration coefficients.
Quantification of the presence of the gas of interest within the gas to be analyzed may be triggered in case the value of the pressure measured along the suction path corresponds to a suction pressure reference value, the quantification of the presence of the gas of interest being performed on the basis of a value of a parameter representative of the mass flow rate along the suction path measured simultaneously with the pressure measurement, which measures the pressure value corresponding to the pressure reference value. Quantification of the presence of the gas of interest may include calculation of the gas proportion of interest according to the following formula:
Figure BDA0001553037020000063
wherein DmIs a parameter representing mass flow rate, and a and B are numerical calibration coefficients; or
M*Dm+ N, wherein DmIs a parameter representing the mass flow rate, M and N are numerical valuesAnd calibrating the coefficients.
Gases of interest may include:
0 to 100% of a first molecule of interest having a certain thermal conductivity, and
from 0 to 100% of the at least one other molecule of interest, the at least one other molecule of interest having a thermal conductivity that ideally differs from the thermal conductivity of the first molecule of interest by at most 10% (preferably at most 5%) under the same conditions,
and the method according to the invention may further comprise:
quantifying the presence of other molecules of interest in the gas to be analyzed by means of at least one gas sensor arranged along the inhalation path, and
quantifying the presence of the first molecule of interest in the gas to be analyzed based on the quantification of the presence of the gas of interest and the quantification of the presence of the other molecules of interest.
The at least one flow path may comprise a dilution path terminating in an opening, and the method according to the invention may comprise: before the gas to be analyzed is sucked, the dilution gas flowing into the sample along the dilution path is discharged.
There is also proposed a method of testing a sample by means of a gas flow, which is preferably implemented in the second aspect of the device according to the invention, and which comprises:
-discharging the leaking gas flowing along a discharge path, the discharge path terminating in an opening communicating with the sample,
-measuring the pressure of the leaking gas along the discharge path,
-measuring a parameter representative of the mass flow rate of the leaking gas along the discharge path, and
-determining the size of the leak in the sample based on the measurement of a parameter representative of the mass flow rate along the discharge path.
The measurement of the parameter representative of the mass flow rate is a measurement preferably made by a mass flow meter using thermal conductivity.
This may be performed by a vent pressure sensor disposed along the vent path between the flow meter and the sample.
The determination of the orifice size may comprise a calculation of the orifice size, wherein the calculation is affine dependent on the square root of a parameter representing the mass flow rate along the discharge path.
The determination of the leak size may also be performed based on the pressure measured along the discharge path. The determination of the leak size may comprise a calculation of the leak size, wherein the calculation is affine dependent on the inverse of the fourth root of the measurement of the pressure along the discharge path. The determination of the leak size may include a determination according to a formula
Figure BDA0001553037020000071
Calculation of the leak size of (2), wherein DmIs a parameter representing the mass flow rate, Pr is the measured pressure, and a and b are numerical calibration coefficients.
The determination of the size of the leak, which is performed on the basis of the value of a parameter representative of the mass flow rate along the exhaust path, measured simultaneously with the pressure measurement, which measures a pressure value corresponding to the pressure reference value, may be triggered in case the value of the pressure measured along the exhaust path corresponds to the exhaust pressure reference value. The determination of the leak size may include a calculation of the leak size according to a formula
Figure BDA0001553037020000072
DmIs a parameter representing the mass flow rate, a*And b is a numerical calibration coefficient.
The at least one flow path may comprise a calibration path passing through the opening and locally narrowing at the measurement aperture, and the method according to the invention may comprise:
-a calibration gas flowing along a calibration path,
-measuring the pressure of the calibration gas along the calibration path,
-measuring a parameter representative of the mass flow rate of the calibration gas along the calibration path,
-determining the size of the measuring orifice based on the step of measuring a parameter representative of the mass flow rate, and
-adjusting the numerical coefficient for calculating the size of the leak if the determined size of the measuring orifice does not correspond to the actual size of the measuring orifice stored by the calculation means.
The method according to the invention may comprise adjusting the total flow rate through the discharge path and the short-circuit path by means of a valve arranged to complete the discharge path through the short-circuit path through the opening and the flow generating means, but not through the flow meter.
Brief description of the drawings and detailed description
Other features and advantages of the invention will become apparent from a reading of the detailed description of the embodiments and examples in no way limiting, and the accompanying drawings, in which:
FIG. 1 is a schematic cross-sectional profile of an apparatus according to the invention, FIG. 1 being a preferred embodiment of the invention and showing the gas flow when the apparatus is in a position for analyzing gas by suction or in a calibration position,
figure 2 schematically shows the pneumatic circuit of the device in figure 1 in a position for analyzing the gas by suction or in a calibration position,
FIG. 3 is a schematic partial section view of a part of the apparatus of FIG. 1, viewed from below, showing the gas flow of the apparatus in a position for analyzing the gas by suction or in a calibration position,
figure 4 schematically shows the pneumatic circuit of the device of figure 1 in a dilution position or in another calibration position,
FIG. 5 is a schematic cross-sectional profile view of the device in FIG. 1, showing the gas flow when the device is in a position for detecting a leak by means of exhaust gas,
FIG. 6 shows schematically the pneumatic circuit of the device of FIG. 1 in a position for detecting a leak by venting,
figure 7 schematically shows the pneumatic circuit of the device in figure 1 in a position of rapid exhaustion by expansion,
figure 8 schematically shows the pneumatic circuit of the device of figure 1 in a position of rupture by venting.
Since these embodiments are in no way limiting, variants of the invention may be considered in particular which comprise only a selection of the features described below in isolation from the other features described (even within a sentence comprising the other features, the selection is isolated) if the selection of the features is sufficient to confer a technical advantage or to distinguish the invention from the prior art. The selection comprises at least one characteristic, preferably a functional characteristic, wherein the at least one characteristic has no constructional detail or has only a part of a constructional detail if the part is sufficient on its own to provide a technical advantage or to distinguish the invention from the prior art.
First, a preferred embodiment of the device 1 according to the invention will be described with reference to fig. 1 to 8. The device 1 is a compact technical sub-assembly that can be mounted in a portable system or included within a stationary device.
The device 1 is a device for testing a sample by means of a gas flow.
The device 1 comprises an opening 2. The opening 2 is an air inlet hole of the hollow of a hollow needle, which is arranged at the center of an air-tight suction cup 24, wherein the air-tight suction cup 24 is arranged to be placed firmly against a sample 13, such as a bag comprising a container or a food product having at least one flexible surface of suitable size that can be penetrated by the needle. The suction cup avoids the use of a sealing diaphragm to perform the test without contaminating the air outside the container.
The device 1 further comprises means 3 for generating a gas flow 25 (gas to be analyzed, dilution gas, leakage gas, calibration gas) in the device 1 along at least one flow path through the opening 2 by means of a mass flow meter 4 and a valve 8, called selector valve.
The valve 8 is a valve with more than two ways (inlet or outlet) and with several possible positions. Each position of the valve 8 corresponds to a particular open configuration for the passage of the airflow 25 or a closed configuration for preventing the airflow 25 from passing between certain inlet and outlet paths of the valve 8.
The valve 8 is preferably a proportional valve (preferably of the drawer type).
The valve 8 is for example a valve manufactured on the basis of a mecalelectron solenoid valve or a Parker valve.
The opening 2 and the valve 8 are common to all flow paths. The microporous filter element 23 is preferably disposed along this common portion of the flow path.
The filter 23 is, for example, a PTFE filter from Millipore or Sartorius.
The generating means 3 comprise a turbine, or more generally a reversible flow generator with speed control to have a controlled flow rate or pressure, such as the reversible flow generator manufactured by Papst corporation.
The generating means 3 are reversible, i.e. they are arranged for equally well generating an intake or exhaust (i.e. in a flow direction opposite to the intake) air flow 25.
The valve 16 and the opening 2 delimit the two ends of each flow path.
The valve 16 is a valve with more than two ways (inlet or outlet) and with several possible positions. Depending on the position of the valve 16, the valve 16 links the generating means 3 to the environment outside the device 1 when in the first position 17 or to the reference gas source 19 when in the second position 18. The valve 16 is, for example, a valve manufactured by Bosch or universal.
The device 1 comprises at least one pressure sensor 5, 6, each pressure sensor 5, 6 being arranged to measure the pressure P of the gas flow 25 along at least one of the flow pathsr. More precisely, the pressure P measured by each sensor 5 or 6rIs the relative pressure (respectively under-pressure or over-pressure) generated by the air flow 25 (respectively sucked into the device 1 or discharged from the device 1) with respect to the absolute pressure measured in the absence of the air flow 25. Each sensor 5, 6 is for example a piezoresistive sensor manufactured by Honeywell, Freescale or sensorportechnics.
The mass flow meter 4 is arranged to measure a parameter representative of the mass flow rate of the gas flow along each flow path. The parameter is typically an electric field strength or a voltage and is preferably proportional to the mass flow rate of the gas flow 25 or linked to the mass flow rate of the gas flow 25 by calculations programmed and/or stored in the computing means 7 of the device. All sensors and control elements 5, 8, 6, 20, 4, 3, 16 are in communication with computing device 7 via an electrical and/or data transmission or control connection (the link indicated by the dashed line in fig. 2). To avoid the further figures being too complex, the calculation and control means 7 are only schematically shown in fig. 2.
In this context, the word "each" is used to denote any unit (e.g. sensor or flow path) chosen individually in the assembly. In the case where the assembly comprises at least one unit (i.e. e.g. "at least one sensor" or "at least one flow path"), there is thus a restrictive case where the assembly comprises a single element (i.e. e.g. a single sensor or a single flow path), and the word "each" denotes the single unit.
The computing means 7 comprise only electronic and/or software technology means, preferably electronic means, and comprise a computer central processing unit, and/or a processor, and/or dedicated analog/digital circuits, and/or software.
The mass flow meter 4 is a mass flow meter utilizing thermal conductivity.
Typically, the mass flow meter 4 comprises a heating element (heat source) and two temperature probes. The heating element is located between the two temperature probes such that the heating element and the two temperature probes are all aligned with the flow direction of the gas flow 25 at the mass flow meter. Based on the temperature change and the heat change between the two temperature probes beside the heat source, the mass flow meter 4 is arranged to determine a parameter representative of the mass flow rate of the gas flow 25 through the flow meter 4 (i.e. the mass of gas passing through the flow path per unit time).
An advantage of a mass flow meter, especially one that utilizes thermal conductivity, is that it has a very fast response time. This therefore enables the diameter of the orifice 22 to be taken or the presence of the gas of interest to be quantified (typical response time is 3 milliseconds) at very high measurement speeds.
The at least one flow path includes:
an inhalation path starting from the opening 2 (i.e. the air flow enters the inhalation path via the opening 2),
a discharge path terminating in an opening 2 (i.e. the gas flow leaves the discharge path via the opening 2), an
A dilution path ending at the opening 2 (i.e. the gas flow leaves the dilution path via the opening 2).
These flow paths are possible in the device 1, depending on the position of the valve 8 and the direction of the air flow 25 generated by the generating means 3. The position of the valve 8 and the direction of the gas flow 25 generated by the generating means 3 (exhaust or intake) at a given moment determine a single flow path (selected from one or zero of the intake path, the exhaust path or the dilution path) through which the gas flow 25 flows in the apparatus 1 at that moment.
All flow paths being closed
For the first position 9 of the valve 8, the valve 8 is closed and the gas flow 25 generated by the device 3 cannot flow along any flow path defined above.
Inhalation path
With reference to fig. 1 to 3, for the second position 10 of the valve 8 and for the generating means 3 of the suction gas flow 25, the means 3 for generating the gas flow 25 are arranged to suck in the gas to be analyzed originating from the sample 13, so that it flows along the suction path into the device 1.
The gas to be analyzed includes, for example:
including one or more molecules (e.g. N)2And O2) Of each of these molecules differs from the thermal conductivity of the other molecules of the gas mixture by at most 10% (preferably at most 5%) under the same temperature and pressure conditions (usually, for the same temperature conditions (measured at pressure P), the thermal conductivity of each of these molecules is at most 10% (preferably at most 5%) (for the same temperature conditions)rDuring which the temperature of the gas flow 25, typically 20 deg.C, and the same pressure conditions (measurement pressure P)r) Respectively has thermal conductivity D in the lower mixed gasiAnd DjEach pair of molecules of (a) to (b),
Figure BDA0001553037020000121
and
Figure BDA0001553037020000122
or preferably
Figure BDA0001553037020000123
And
Figure BDA0001553037020000124
) (ii) a This threshold, optimally fixed at 5% or 10%, may in other embodiments also be greater than 10% (20%, 30%, etc.), but the higher the threshold, the poorer the resolution of the device according to the invention; and
comprising only one or more molecules (e.g. NO)2And/or CO2) 0 to 100% of the gas of interest, the difference in thermal conductivity between these molecules under the same temperature and pressure conditions is less than or equal to 10% (preferably less than or equal to 5%) (typically, for a thermal system at the same temperature conditions (measured at pressure P)rDuring which the temperature, typically 20 deg.C, and pressure conditions (measured pressure P) of the gas stream 25r) Respectively have a thermal conductivity C in the gas of interestiAnd CjEach pair of molecules of (a) to (b),
Figure BDA0001553037020000125
and
Figure BDA0001553037020000126
or preferably
Figure BDA0001553037020000127
And
Figure BDA0001553037020000128
). The threshold, which is optimally set to 5% or 10%, may in other embodiments also be set to more than 10% (20%, 30%, etc.), but the higher the threshold, the poorer the resolution of the device according to the invention. The thermal conductivity of each molecule of the gas of interest differs from the thermal conductivity of each molecule of the mixed gas by at least 20%, preferably at least 30%, under the same temperature and pressure conditions (typically, under the same temperature conditions (measured under pressure, P)rDuring which the temperature, typically 20 deg.C, and the pressure conditions (measured pressure P) of the gas stream 25r) For having thermal conductivity CiAnd has a thermal conductivity DiEach molecule of the mixed gas of (a) and (b),
Figure BDA0001553037020000129
and
Figure BDA00015530370200001210
or preferably
Figure BDA0001553037020000131
And
Figure BDA0001553037020000132
). This difference of at least 20% or 30% affects the accuracy of the device 1; the larger the difference, the more the gas of interest is differentiated and the less use of electron amplification; this threshold, which is optimally set to 20% or 30%, can in other embodiments also be set to less than 20%, but the smaller the threshold, the poorer the resolution of the device according to the invention, or the higher the need for other redundant technical means for the implementation of the differentiated high-performance electronics or devices described in other measurement scales will be.
In the device 1, the above-mentioned suction path narrows locally at the measuring orifice 14. The measuring hole 14 is a hole made in the plate 15. The plate 15 is typically made of stainless steel. The plate 15 is removable so that it can be replaced, typically in the event of wear of the holes 14 or in order to change the size of the holes 14 in the device 1. The pores 14 have a known size, typically 5 μm to 15 μm in diameter. The gas flow passes through a second orifice 21 of larger diameter (typically about 2mm) than the measuring orifice 14. The thickness of the perforated plug 15 is a factor for adjusting the reduction in the load sought and is much smaller (typically about 10 times smaller) than the size of the microperforation openings 14.
The aperture 14 is a passage for the air flow 25 in the device 1 with a minimum aperture area (per unit surface area perpendicular to the direction of the air flow 25) compared to the rest of the suction path as a whole, even preferably compared to the rest of the discharge path and the dilution path. All locations along the suction path (and even preferably the discharge path and the dilution path) obviously have, apart from the apertures 14 themselves, an aperture area (per unit surface area perpendicular to the direction of the airflow 25) at least 5 times greater than the aperture area (per unit surface area perpendicular to the direction of the airflow 25) of the apertures 14.
The shape of the aperture 14 is circular.
At least one pressure sensor 5, 6 comprises a pressure sensor arranged to measure the pressure P of the gas to be analyzed along the suction pathrOr more precisely the negative pressure, directly linked to the suction of the turbine 3, a first pressure sensor 6 (called suction pressure sensor), the pressure PrPreferably but not limitatively comprised between 20 and 500mbar or wider (depending on the capacity of the turbine 3 comprised between 4 and 500mbar or between 4 and 1000mbar or wider).
The mass flow meter 4 is arranged to measure a parameter representative of the mass flow rate of the gas to be analysed along the suction path.
Based on the measured value of the parameter representative of the mass flow rate of the gas to be analyzed, the calculation means 7 are arranged to quantify the presence of the gas of interest in the gas to be analyzed (this quantified presence is generally the proportion of the gas of interest in% of the gas to be analyzed, or in moles per liter of the gas to be analyzed, or in the form of a volume of the gas of interest (for example in milliliters)).
The calculation means 7 is arranged to quantify the presence of the gas of interest in the form of a calculation of the proportion or volume of the gas of interest, wherein the calculation depends on the diameter of the measuring orifice 14. In other words, if the diameter or width of the orifice 14 changes (by program, command or adjustment knob, etc.) without indicating to the device 1 a change in its diameter or width, the calculation of the proportion or volume of the gas of interest by the device 1 will become inaccurate.
For best measurement accuracy, the first suction pressure sensor 6 is arranged along the suction path between the opening 2 and the measurement orifice 14.
The mass flow meter 4 is disposed along the suction path so that the measuring hole 14 is disposed along the suction path between the opening 2 and the mass flow meter 4.
The inventionThe inventors have found experimentally that excellent measurement accuracy for the size of a narrowed orifice (e.g., 14 or 22) in a flow can be obtained by passing an air stream 25 (typically air) through the orifice and measuring the diameter φ of the orifice using the following equationcalTo realize that:
Figure BDA0001553037020000141
(hereinafter referred to as "first formula")
Wherein DmIs a parameter representing the mass flow rate of the gas stream through the orifice, PrIs the pressure of the gas stream, and X and Y are numerical calibration coefficients.
With respect to the measured value DmThe mass flow meter 4 is optimized for one or more gases having a default value for thermal conductivity. For gases having a thermal conductivity different from the default value, a correction factor will be applied.
For example, in the case of a mass flow meter 4 of the Honeywell AWM series, if the air flow is air and/or N2And/or O2And/or NO and/or CO, the flow rate D measured by the mass flow meter 4mMust be multiplied by a factor of 1 (non-correction factor), and DmMust be multiplied by a correction factor Kcal1.35 (if the gas stream is CO)2And/or N2O flow), or factor Kcal0.5 (for He), Kcal0.7 (for H)2)、Kcal0.95 (for Ar), and Kcal1.1 (for CH and/or NH)3) Etc. (which may typically be referenced to a user indication of the model for the flow meter 4 being used).
It is assumed that the gas to be analyzed is O originating from the sample 13 and circulating in the apparatus 1 along the suction path2And CO2A mixture of (a); it is assumed that the two gases are known to each constitute a mixture in a ratio of 0 to 100%, but the ratio of the two gases is unknown. Actual diameter phi of the reference hole 14rIs 100 μm.
If the calculation means 7 calculate the diameter phi of the hole 14 of 100 μm using the first formula described earlierrThe calculating means 7 thus being based on these gasesWhich is considered to be the gas of interest infers O in the mixture2Is 100%, or CO in the mixture2The ratio of (B) is 0%.
If the computing means 7 make use of what has been described previously for phirCalculates the diameter of the holes 14 of 135 μm, the calculation means 7 thus deducing O from the mixture on the basis of which of these gases is considered to be the gas of interest2Is 0%, or CO in the mixture2The proportion of (B) is 100%.
In general, if the computing means 7 make use of what has been described previously for phirIs calculated by the formula (II)calFrom the gas in question (using the formula hereinafter referred to as the "second formula") to infer CO in the mixture2In a ratio of
Figure BDA0001553037020000151
Or O in the mixture2In a ratio of
Figure BDA0001553037020000152
KcalCorrection factor for gas of interest (at CO) as explained earlier2In case of (2) Kcal＝1.35)。
The calculation means 7 do not have to go through these two steps, which consist in calculating the diameter of the holes 14 (first step, first formula) and then deducing the proportion of the gas of interest (second step, second formula), but can directly calculate this proportion in a single calculation combining these two steps and therefore these two formulas.
The calculation means 7 are thus arranged to quantify the presence of the gas of interest in the form of a calculation of the proportion or volume of the gas of interest, the calculation preferably being affine dependent on the parameter D representing the mass flow ratemThe square root of (a).
Alternatively, in the case of inaccuracies of a limited expansion of the first formula to the first order, the calculation means 7 are arranged to quantify the presence of the gas of interest in the form of a calculation of the proportion or volume of the gas of interest, which calculation is affine dependent on the parameter representing the mass flow rate.
Generally, in the case of a finite expansion of the first formula to the Z order (Z being an integer greater than or equal to 1), the calculation means 7 quantify the presence of the gas of interest in the form of a polynomial of degree Z of the parameter representative of the mass flow rate.
In this context, two variants of the invention are envisaged which can be optionally combined within a single device 1.
In a first variant, the calculation means 7 are arranged to also pass the pressure P measured by the suction pressure sensorrQuantifying the presence of a gas of interest:
preferably, the calculation means 7 are arranged to quantify the presence of the gas of interest in the form of a calculation of the proportion or volume of the gas of interest, which calculation depends affine ly on the inverse of the fourth root of the pressure measured by the suction pressure sensor. The proportion or volume of the gas of interest is typically calculated according to the following formula:
Figure BDA0001553037020000161
wherein DmIs a parameter representing the mass flow rate, P, measured by the mass flow meter 4rIs the pressure measured by the suction pressure sensor 6, and a and B are numerical calibration coefficients.
Optionally, an approximation can be made. For example, the calculation means 7 may be arranged to quantify the presence of the gas of interest in the form of a calculation of the proportion or volume of the gas of interest, wherein the calculation is affine dependent on the inverse of the pressure measured by the suction pressure sensor 6. The proportion or volume of the gas of interest is typically calculated according to the following formula:
Figure BDA0001553037020000162
wherein DmIs a parameter representing the mass flow rate measured by the mass flow meter 4, PrIs the pressure measured by the suction pressure sensor 6, and M and N are numerical calibration coefficients.
In a second variant, the pressure P measured by the suction pressure sensor 6rIs not considered inWithin the formula for calculating the proportion or volume of gas of interest, but serving as a trigger: the calculation means 7 are arranged to trigger the quantification of the presence of the gas of interest for the pressure P measured by the suction pressure sensor 6 corresponding to a suction pressure reference valuerBased on a value D of a parameter representative of the mass flow rate measured simultaneously with the pressure measurement, the calculation means 7 being arranged to calculate the value ofmThe presence of the gas of interest is quantified, wherein the pressure measurement measures a pressure value corresponding to a suction pressure reference value. The calculation means 7 is then arranged to quantify the presence of the gas of interest in the form of calculating the proportion or volume of the gas of interest:
-preferably according to the formula:
Figure BDA0001553037020000163
wherein DmIs a parameter representing the mass flow rate measured by the flow meter 4, and a and B are numerical calibration coefficients.
-optionally according to the formula:
M*Dm+ N or any D as explained beforemAny other polynomial of degree Z, where DmIs a parameter representing the mass flow rate measured by the flow meter 4, and M and N are numerical calibration coefficients.
According to the invention, all calibration factors A, B, M, N, A, M, a, b, a are stored and predefined by the calculation means 7, the apparatus 1 being generally calibrated with samples 13 having known proportions of different gases or samples 13 each provided with a leak orifice of known size.
The value of each calibration factor depends on the gas in question. For example, one can assume CO with the gas of interest2Mixed gas O2Or with a gas of interest CH4+NH3Mixed gas He, etc.
The apparatus 1 thus comprises an interface arranged to define a mixed gas and a gas of interest, and the calculation means 7 is arranged to select a value of the calibration factor in dependence on the defined mixed gas and the gas of interest.
The suction path continues through the opening 2, the filter 23, the pressure sensor 5, the valve 8, the pressure sensor 6, the measuring hole 14, the gas sensor 20, the passage hole 21, the flow meter 4, the generating means 3 and the valve 16.
The apparatus 1 further comprises at least one sensor 20, the sensor 20 being arranged to quantify the presence of a gas consisting of a given molecule, the thermal conductivity of which does not differ from the thermal conductivity of another gas or molecule present.
Calculating means 7 (e.g. when the gas mixture is O)2And the gas of interest is CO2+NO2In the case of a mixture) is also arranged to provide a first molecule of interest (e.g., CO in this case) in the gas of interest that will have a certain thermal conductivity2) To this end, the device 1 comprises, along the suction path, at least one gas sensor 20 (for example NO in this case)2A sensor, such as one manufactured by City technology), the at least one gas sensor 20 being arranged to sense at least one other molecule of interest (e.g., NO in this case)2) In (e.g. in% or in mol.l)-1In proportion of units, or volume), the thermal conductivity of which differs by no more than 10% from the first molecule of interest under the same temperature and pressure conditions, the calculation means 7 being arranged to base (simple subtraction) on the gas of interest (CO)2+NO2) Quantification of the presence of and other molecules of interest (NO)2) Quantifying the presence of (a) a first molecule of interest (CO)2) Presence of (a) is quantified.
For example, if the following results are measured:
gas of interest CO2+NO2In a proportion of 20% of the gas to be analyzed
2Ratio of NO5% of the gas to be analyzed
Then the following results are inferred:
2proportion of the mixed gas (O)＝100-CO2+NO2In a proportion of 80% of the gas to be analyzed
2Proportion of COGas to be analyzed15% of the body
The sensor 20 is arranged along the suction path such that the measuring orifice 14 is arranged between the opening 2 and the sensor 20. The sensor 20 is provided in the measurement chamber along a suction path between the measurement hole 14 and a passage hole 21 wider than the measurement hole 14.
The at least one sensor 20 may also be O2Sensor or other sensors (e.g. O)2Sensor and NO2Sensor assembly), for example if the mixed gas includes O2And N2In order to distinguish between the two molecules.
Dilution path
With reference to fig. 4, the means 3 for generating a gas flow 25 are arranged to discharge the dilution gas along the dilution path, for the same position of the valve 8 as the suction path (second position 10), and for the means 3 for generating a discharge gas flow 25.
The dilution path thus corresponds to the suction path but the airflow 25 passes therethrough in the opposite direction.
For the dilution path, valve 16 is in a second position 18 that links device 3 to a gas source 19. The dissolved gas is thus a reference gas from a source 19, typically a gas cartridge.
The dilution path is used to increase the volume of gas to be analysed in the sample 13.
Dilution route example 1
Suppose that sample 13 initially included only CO as the initial gas2+NO2Not including O2But the amount of the mixture is too small to draw the mixture into the device 1 to fill all the suction paths: therefore, CO cannot be determined in this case2And NO2The ratio of (a) to (b). On the other hand, if derived from O of the gas source 192Is introduced into the sample 13 through the dilution path, the sample 13 then comprises CO2+NO2+O2And the amount of the mixture is sufficient to perform the measurement. After dilution as described above, CO2、NO2And O2The ratio of (c) can be determined. CO before dilution2In a ratio of (A) to (B) and NO2In a ratio ofTo be inferred thereby.
For example, the following results were measured:
CO2+NO2the proportion of (A) is 20% of the gas to be analyzed after dilution
NO2The proportion of (A) is 5% of the gas to be analyzed after dilution
The following result is deduced therefrom:
O2in a ratio of 100-CO2+NO2The proportion of (A) is 80% of the gas to be analyzed after dilution
CO2The proportion of (A) is 15% of the gas to be analyzed after dilution
Namely:
2ratio of NO25% of the initial gas before dilution
2Proportion of CO75% of the initial gas before dilution
Dilution route: example 2
Suppose that sample 13 initially includes only N as the initial gas2And O2But in an amount too small to draw the mixture into the device 1 to fill all inhalation paths: therefore, O cannot be determined in this case2And N2Proportion or volume of (c). On the other hand, if the CO originates from the gas source 192Is introduced into the sample 13 through the dilution path, the sample 13 then comprises CO2+N2+O2And the amount of the mixture is sufficient to perform the measurement. By using the volume of gas injected or the volume of gas inhaled, CO2、N2And O2The ratio of (c) can be determined after dilution as described previously. Then CO before dilution2And N2The ratio of (c) can be deduced therefrom.
-an initial phase: assume that the volume of gas contained is V1 (this problem is typically encountered when the available volume of the bag is less than 3 ml). This volume V1 is not known in the initial stage. Volume V1 contains most of N2And a trace amount of O2Trace amount of O2Cannot be measured due to the available volume in the container.
-dilution: the dilution of the volume is at least sufficient to excite O by injection2The volume V2 of the sensor (labeled 20) is 10ml of 100% CO2To be implemented.
Then a volume of V2 was again aspirated.
The proportions given are:
mixture O2+CO2+N21.34 instead of 1.35 (ref N)2+O2Air)
N present in the diluted mixture2+O2The amount of (100-1.34 × 100/1.35) × V2 ═ 0.00296 × V2 ═ 0.0296ml
CO Included in V22The volume of (A) is V2-0.037% x V2 ═ 9.97ml
O in V22The concentration of (B) became 99.704%
O in diluted mixture V2 given by sensor 2020.01%, namely 0.001ml
In the initial volume V1O2The ratio of (1) to (2) is 0.001X 100/0.0296 to 3.378%
And from this it can be concluded that the volume V1: (100-99.704). times.10 ml-2.96 ml
Discharge path
With reference to fig. 5 and 6, for the third position 11 of the valve 8 and for the generating means 3 of the exhaust gas flow 25, the means 3 for generating a gas flow are arranged to exhaust the leakage gas along the exhaust path.
Depending on the position of the valve 16, leaking gas (preferably O)2Or air) from an external environment or source 19.
At least one pressure sensor comprises a pressure sensor arranged to measure the pressure P of leaking gas along the discharge pathrWithin the limits of the reduction of the load in the pneumatic circuit and of the pressure resistance of the elements constituting the invention, and in any case the pressure value P of the leaking gasrPreferably but not limitatively between 20 and 500mbar, or more broadly between 4 and 500mbar, or between 4 and 1000 mbar.
The mass flow meter 4 is arranged to measure a parameter representative of the mass flow rate of the leaking gas along the discharge path.
The calculation means 7 are arranged to determine the size of the leak orifice 22 of the sample 13 into which the leaking gas evacuated by the apparatus 1 is introduced, based on the measured value of the parameter representative of the mass flow rate.
An exhaust gas pressure sensor 5 is provided along the exhaust path between the flow meter 4 and the opening 2.
The calculation means 7 are arranged to determine the size of the leak 22, preferably in the form of a calculation which is affine dependent on the square root of the parameter representing the mass flow rate (see the first formula described earlier).
Alternatively, in the case of inaccuracies in which the first formula is expanded to a first order to a limited extent, the calculation means 7 are arranged to determine the size of the leakage orifice 22 in the form of a calculation which is affine dependent on a parameter representing the mass flow rate.
In general, the calculation means 7 are arranged to determine the size of the orifice 22 in the form of a polynomial of degree Z of a parameter representative of the mass flow rate, in the case of a finite expansion of the first formula to the order Z (Z being an integer greater than or equal to 1).
In this context, two variants of the invention are envisaged which can be optionally combined within a single device 1.
In a first variant, the calculation means 7 are arranged to determine the size of the hole 22 also on the basis of the measured value of the pressure measured by the exhaust pressure sensor 5, for example in the form of a calculation of the inverse of the fourth square root, which preferably depends affine on the pressure measured value. Typically, the calculation means 7 are arranged to determine the size of the hole 22 according to the following formula:
Figure BDA0001553037020000211
wherein DmIs a measurement value representing the mass flow rate measured by the flow meter 4
Parameter of (A), PrIs the pressure measured by the exhaust pressure sensor 5, and a and b are numerical calibrations
And (4) the coefficient.
According to the invention, the diameter of the leak hole 22 can be measured, which is typically a minimum of up to 0.05 μm.
In the second modification, the pressure P measured by the exhaust pressure sensor 5rNot considered in the formula for calculating the size of the leak 22, but acts as a trigger: the calculation means 7 are arranged to trigger the determination of the size of the leak 22 for a value of the pressure measured by the discharge pressure sensor 5 corresponding to a reference value of the discharge pressure, the calculation means 7 being arranged to be based on a signal representative of the mass flow rate D measured simultaneously with the pressure measurementmDetermines the size of the orifice 22 and the pressure measurement measures a pressure value corresponding to the suction pressure reference value. The calculation means 7 are for example arranged to determine the size of the hole 22 according to the following formula:
Figure BDA0001553037020000212
wherein DmIs a parameter representing the mass flow rate measured by the flow meter 4
Numbers, a and b are numerical calibration coefficients.
The discharge path is divided into two parts which are separated before the measuring orifice 14 and rejoined after the measuring orifice 14:
the first part passes the measuring orifice 14 (and comprises the sensor 6 and the measuring chamber comprised between the measuring orifice 14 and the passage orifice 21),
the second portion does not pass through the measuring orifice 14, so that the measuring orifice 14 does not restrict the flow rate of the exhaust air flow 25 in the exhaust path.
The discharge path continues through valve 16, generating means 3, flow meter 4, two parts that are split before measuring hole 14 and joined after measuring hole 14, valve 8, pressure sensor 5, filter 23 and opening 2.
Calibration path
The at least one flow path comprises a calibrated path through the opening 2, which corresponds to an inhalation path or a dilution path. The calibration path narrows locally at the measurement aperture 14. When the generating means 3 generate a suction or discharge flow 25 (calibration gas) in this calibration path and the opening 2 is not connected to the closed sample 13 (the opening 2 is preferably open to the external environment), the computing means 7 are arranged to:
1) based on a parameter D representative of the mass flow rate measured by the flowmeter 4mAnd determining the size of the measuring orifice 14 on the same principle as the determination of the size of the leak orifice 22 described previously, an
2) If the determined dimension phi of the measuring holecalWith the actual size phi of the measuring hole 14 stored by the calculating means 7rNot, the numerical coefficients (generally a, b, a, etc.) used to calculate the size of the leak 22 are adjusted,
3) the above steps 1) and 2) are optionally repeated until the determined size of the measuring hole 14 corresponds to the actual value of the measuring hole 14 stored by the calculating means 7 within an allowable error percentage.
Short-circuit path
Referring to fig. 7 and 8, the valve 8 in its fourth position 12 is arranged to complete the discharge path by a short-circuit path through the opening 2 and the flow generating means 3, but not through the flow meter 4 (so that the short-circuit path does not form part of the previously defined flow path). The valve 8 is arranged to regulate the total flow rate through the discharge path and the short-circuit path. This allows a greater flow rate DmAnd thus makes it possible to measure other ranges of diameters of the leak hole 22 or to rapidly expand the specimen 13 to test its breaking strength by sustained fatigue or stress phenomena. When the valve 8 opens the short-circuit path, the calculation means 7 are arranged to base the flow rate measurement D along the discharge path measured by the mass flow meter 4 onmThe total flow rate through the drain path and the short circuit path is inferred.
In general, when the valve 8 opens the short-circuit path, the computing means 7 applies the mass flow rate D measured by the mass flow meter 4 by means of a calibration factormTo obtain the total flow rate through the drain path and the short circuit path. Alternatively, the calculation means 7 modify the values of the calibration coefficients a and a during the determination of the size of the leak orifice 22 so as to increase the total flow rate through the bleed and short-circuit paths above the parameter D measured by the flowmeter 4mThe fact of the measured value ofTaking into account, wherein the parameter DmRepresenting the mass flow rate of the leaking gas along the exhaust path.
An example of a method whose sequence can be modified according to the invention implemented by the device 1 in fig. 1 to 8 will now be described. Gas species (O) as mentioned2、CO2、NO2Etc.) are used for illustrative purposes only and are obviously subject to change.
Dilution of
Firstly, before the gas to be analyzed is aspirated, the method according to the invention comprises the evacuation (through the device 3) of the dilution gas (CO originating from the source 19) flowing along the dilution path into the sample 132) Wherein the sample 13 comprises a starting gas (CO)2And NO2Mixtures of (b) that preferably, but not necessarily, includes the gas of interest.
Gas analysis
After dilution, the method according to the invention comprises the aspiration (through the device 3) of the gas to be analyzed (O) originating from the sample 132+CO2+NO2) The gas to be analyzed that is sucked in flows along a suction path that starts at the opening 2 and narrows locally at the measuring orifice 14.
During inhalation, the method according to the invention simultaneously comprises:
measuring the pressure P of the gas to be analyzed along the suction path by means of the sensor 6r(more precisely, the negative suction pressure, which is negative a priori but is considered as an absolute value for the calculation), depending on the capacity of the turbine 3, PrPreferably but not limitatively comprised between-20 mbar and-500 mbar or more broadly comprised between 4mbar and 500mbar or between 4mbar and 1000mbar or more;
measuring a parameter representative of the mass flow rate of the gas to be analyzed along the suction path by means of the flow meter 4.
The method according to the invention also comprises the step of treating the gas to be analyzed (O) by means of the calculation means 7 on the basis of the last measurement of the parameter representative of the mass flow rate2+CO2+NO2) Gas of interest (CO)2+NO2) Presence of (a) is quantified: for example, 2CO+ 2the NO ratio is 20% of the gas to be analyzed after dilution. Quantification of the presence of the gas of interest includes the calculations described for the description of the apparatus 1.
Gases of interest (CO)2+NO2) Comprising a first molecule of interest (CO) having a certain thermal conductivity2) 0 to 100% of (a), and other molecules of interest (NO)2) 0 to 100% of (a), wherein the other molecule of interest (NO)2) Having a thermal conductivity which differs from the thermal conductivity of the first molecule of interest by at most 10% (preferably at most 5%) under the same temperature and pressure conditions.
The method according to the invention also comprises (simultaneously with the measurement of the pressure and the measurement of the parameter representative of the mass flow rate) introducing the gas to be analyzed (O) through the sensor 202+CO2+NO2) Other molecules of interest (NO)2) Presence quantification of (a): for example 2The NO ratio is 5% of the gas to be analyzed after dilution。
The method according to the invention further comprises: based on the gas (O) to be analysed2+CO2+NO2) Gas of interest (CO)2+NO2) Quantification of the presence of and gas (O) to be analyzed2+CO2+NO2) Other molecules of interest (NO)2) Quantification of the presence of gas (O) to be analyzed2+CO2+NO2) First molecule (CO) of interest2) Presence quantification of (a): for example 2Diluting the mixture with CO 15% of the analyzed gas。
The method according to the invention further comprises: based on the gas (O) to be analysed2+CO2+NO2) First molecule of interest (CO)2) Quantification of the presence of and gas (O) to be analyzed2+CO2+NO2) Other molecules of interest (NO)2) Quantification of the Presence of the initial gas (CO)2+NO2) First molecule (CO) of interest2) Presence quantification of (a): for example 2Ratio of CO to initial gas 75％。
The method according to the invention further comprises: based on the gas (O) to be analysed2+CO2+NO2) First molecule of interest (CO)2) Quantification of the presence of and gas (O) to be analyzed2+CO2+NO2) Other molecules of interest (NO)2) Quantification of the Presence of the initial gas (CO)2+NO2) Other molecules of interest (NO)2) Quantification of the presence of (c): for example 2Ratio of NO to initial gas 25％。
Mechanical testing of sample 13 was then performed.
Calibration of leak measurements
The method according to the invention comprises a flow (generated by means of the device 3) of a calibration gas (preferably external air or gas coming from a source 19) along a calibration path, simultaneously with which:
1) measuring the pressure P of the calibration gas along the calibration path by means of the sensor 5 or 6rThe pressure P ofrPreferably but not limitatively between 20 and 500mbar, or more broadly between 4 and 500mbar, or between 4 and 1000mbar,
2) a parameter representative of the mass flow rate of the calibration gas along the calibration path is measured by the flow meter 4,
3) determining, by means of the computing means 7, the size of the measuring orifice 14 on the basis of the last measurement of the parameter representing the mass flow rate, an
4) If the determined dimension phi of the measuring hole 14 is determinedcalIn a way that does not correspond to the actual dimensions of the measuring opening 14 stored by the computing device 7, the computing device 7 adjusts the calibration factors a, b for calculating the dimensions of the leakage opening 22, and
5) optionally repeating steps 1 to 4 as previously described.
Leak measurement
The method according to the invention comprises discharging leaking gas (preferably outside air or gas from source 19 or tracer gas which can localize the leak, which is a colorant or can be measured by other external means) flowing along a discharge path terminating at opening 2.
During the venting, the method according to the invention simultaneously comprises:
measuring the pressure P of the leaking gas along the discharge path by means of the sensor 5rThis pressure P is in any case within the limits of the load reduction of the pneumatic circuit and within the limits of the pressure resistance of the elements constituting the inventionrPreferably but not limitatively between 20 and 50mbar, or more broadly between 4 and 500mbar, or between 4 and 1000 mbar.
-measuring a parameter representative of the mass flow rate of the leaking gas along the discharge path by means of the mass flow meter 4.
The method according to the invention comprises determining, by means of the computing means 7, the size of the leak 22 in the sample 13 on the basis of the final measurement of the parameter representative of the mass flow rate.
Determining the size of the leak 22 includes calculations as described for the description of the device 1.
If the weep hole 22 is too large, the flow rate of the leaking gas must be increased in an attempt to achieve the setpoint pressure. The method according to the invention comprises adjusting the total flow rate through the discharge path and the short-circuit path by means of a valve 8, wherein the valve 8 is arranged to complete the discharge path through the short-circuit path flowing through the opening and the flow generating means without passing through the flow meter, which valve opens the short-circuit path according to the opening of adjustable size.
The method according to the invention comprises the following steps: when the valve 8 opens the short-circuit path, the total flow rate through the discharge path and the short-circuit path is determined by the device 7 on the basis of the measurement of the flow rate along the discharge path.
More specifically, the calculation means 7 modify the values of the calibration coefficients a and a during the determination of the size of the leak orifice 22 so as to increase the total flow rate through the discharge path and the short-circuit path above the parameter D measured by the flowmeter 4mTaking into account the fact that the parameter D ismRepresenting the mass flow rate of the leaking gas along the exhaust path.
Strength/fracture test
After the leak orifice 22 is sized, the gas flow rate is raised to a high value, optionally at a controlled flow rate, to perform a rupture test on the sample 13 with the desired kinetics.
It should be noted that in the method according to the invention, the sample 13 may be subjected to extreme external mechanical stresses, such as a restrictive overwrap, atmospheric pressure, immersion in a fluid, etc.
It should also be noted that the various steps of the method may be reversed, or may be performed simultaneously or alternatively. For example, the calibration step does not have to precede the leak measurement. Similarly, the leak measurement is completely independent of the gas analysis, and the leak measurement may be performed prior to the gas analysis or without the gas analysis. In a preferred case, to save time, the leakage measurement may be performed simultaneously with the dilution, preferably once the equilibrium pressure is reached, the exhausted dilution gas also acting as the exhausted leakage gas.
Of course, the invention is not limited to the examples that have been described, and various modifications can be made to these examples without exceeding the scope of the invention.
Of course, the different features, forms, variants and embodiments of the invention can be combined with one another in various combinations, compatible or not mutually exclusive. In particular, all the variants and embodiments described above can be combined.

Claims (20)

1. An apparatus for testing a sample (13) by means of a gas flow (25), comprising:
-an opening (2),
-means (3) for generating an air flow (25) in the device along at least one flow path through the opening,
-at least one pressure sensor (5, 6), each arranged to measure the pressure of the gas flow along at least one flow path, an
-a mass flow meter (4) arranged to measure a parameter representative of a mass flow rate of the gas flow along each flow path,
the method is characterized in that:
-the at least one flow path comprises a discharge path terminating at the opening,
-the means for generating the gas flow are arranged to discharge leakage gas along the discharge path,
-the at least one pressure sensor comprises a degassing pressure sensor (5) arranged to measure a pressure of the leaking gas along the discharge path,
-the mass flow meter is arranged to measure a parameter representative of a mass flow rate of the leaking gas along the discharge path, and
-the device further comprises calculation means (7) arranged to determine the size of a leak (22) based on a measured value of said parameter representative of the mass flow rate along said discharge path,
wherein the mass flow meter is a mass flow meter utilizing thermal conductivity.
2. The apparatus of claim 1,
the exhaust pressure sensor is disposed along the exhaust path between the mass flow meter and the opening.
3. Apparatus according to claim 1, wherein the calculation means is arranged to determine the size of the orifice in the form of a calculation which is affine-related to the square root of the parameter representing the mass flow rate along the discharge path.
4. An arrangement according to claim 1, characterised in that the calculation means are arranged to determine the size of the leak also on the basis of a measurement of the pressure along the discharge path measured by the exhaust pressure sensor.
5. Apparatus according to claim 4, wherein the calculation means is arranged to determine the size of the leak in the form of a calculation which is related to the inverse affine of the fourth root of the measurement of the pressure along the discharge path.
6. The apparatus of claim 5, wherein the computing device is configured to determine the size of the leak according to the formula:
Figure FDA0002836592280000021
wherein DmIs a parameter representing the mass flow rate, PrIs the pressure measured by the exhaust pressure sensor, and a and b are numerical calibration coefficients.
7. The apparatus of claim 1, wherein the computing device is configured to trigger the determination of the size of the leak for a value of the pressure along the exhaust path measured by the exhaust pressure sensor corresponding to an exhaust pressure reference value, the computing device being configured to determine the size of the leak based on a value of a parameter representative of a mass flow rate along the exhaust path measured concurrently with a pressure measurement, wherein the pressure measurement is a measurement of the pressure value corresponding to the exhaust pressure reference value.
8. The apparatus of claim 7, wherein the computing device is configured to determine the size of the leak according to the formula:
Figure FDA0002836592280000022
wherein DmIs a parameter representing the mass flow rate, and a and b are numerical calibration coefficients.
9. The device according to claim 1, characterized in that the at least one flow path comprises a calibration path through the opening and within the device, which locally narrows at a measurement orifice (14),
wherein the computing device is configured to:
-determining the size of the measurement aperture based on a measured value of a parameter representative of the mass flow rate along the calibration path, and
-adjusting the calibration factor for calculating the leak size if it is determined that the size of the measurement hole does not correspond to the actual size of the measurement hole stored by the calculation means.
10. An apparatus according to claim 1, characterized in that the apparatus comprises a valve (8) arranged to complete the exhaust path by a short-circuit path through the opening and the means for generating a gas flow, but not through the mass flow meter, the valve being arranged to adjust the total flow rate through the exhaust path and the short-circuit path.
11. A method for testing a sample by gas flow, the method comprising:
-venting the leakage gas flowing along a venting path terminating in an opening (2) communicating to the sample (13),
-measuring the pressure of the leaking gas along the discharge path,
-measuring a parameter representative of the mass flow rate of leaking gas along the discharge path, and
-determining the size of a leak (22) in the sample based on the measurement of the parameter representative of the mass flow rate along the discharge path,
wherein the step of measuring a parameter representative of the mass flow rate is a measurement by a mass flow meter (14) using thermal conductivity.
12. The method of claim 11,
the measurement of the pressure is performed by an exhaust pressure sensor (5) arranged along an exhaust path between the mass flow meter and the sample.
13. The method of claim 11, wherein the step of determining the size of the weep hole comprises calculating the size of the weep hole, wherein the calculation is affine related to the square root of the parameter representing the mass flow rate along the discharge path.
14. The method of claim 11, wherein the step of determining the size of the leak is further performed based on a pressure measured along the discharge path.
15. The method of claim 14, wherein the step of determining the size of the leak comprises calculating the size of the leak, wherein the calculation is related to the inverse affine of the fourth root of the measurement of the pressure along the discharge path.
16. The method of claim 15, wherein the step of determining the size of the leak comprises calculating the size of the leak according to the formula:
Figure FDA0002836592280000041
wherein DmIs a parameter representing the mass flow rate, Pr is the measured pressure, and a and b are numerical calibration coefficients.
17. The method according to claim 11, characterized in that the step of determining the size of the leak is triggered in case the value of the pressure measured along the exhaust path corresponds to an exhaust pressure reference value, and the step of determining the size of the leak is performed on the basis of the value of the parameter representative of the mass flow rate along the exhaust path measured simultaneously with the pressure measurement, which is the measurement of the pressure value corresponding to the pressure reference value.
18. The method of claim 17, wherein the step of determining the size of the leak comprises calculating the size of the leak according to the formula:
Figure FDA0002836592280000042
wherein DmIs a parameter representing the mass flow rate, a*And b is a numerical calibration coefficient.
19. The method of claim 11, comprising generating an airflow along at least one flow path through the opening, and the at least one flow path comprises a calibrated path through the opening and locally narrowed at a measurement aperture, and further comprising:
-a calibration gas flowing along the calibration path,
-measuring the pressure of the calibration gas along the calibration path,
-measuring a parameter representative of a mass flow rate of a calibration gas along the calibration path,
-determining the size of the measurement orifice based on the measurement of the parameter representative of the mass flow rate, and
-adjusting the numerical coefficient for calculating the size of the leak if the determined size of the measuring orifice does not correspond to the actual size of the measuring orifice stored by the calculation means.
20. The method of claim 11,
the method comprises adjusting the total flow rate through the discharge path and a short-circuit path through the opening and the means for generating a gas flow but not through a mass flow meter by means of a valve (8) arranged to complete the discharge path through the short-circuit path.
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